CN109181661A - A kind of oil field sealing agent and preparation method thereof - Google Patents
A kind of oil field sealing agent and preparation method thereof Download PDFInfo
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- CN109181661A CN109181661A CN201811197297.XA CN201811197297A CN109181661A CN 109181661 A CN109181661 A CN 109181661A CN 201811197297 A CN201811197297 A CN 201811197297A CN 109181661 A CN109181661 A CN 109181661A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/44—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing organic binders only
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Abstract
The invention discloses a kind of oil field sealing agents and preparation method thereof.The oil field sealing agent the preparation method comprises the following steps: starch is taken to be placed in water gelatinization, acrylamide and glycine betaine are added into gained mixture, it is stirring evenly and then adding into initiator and crosslinking agent, is stirred evenly, resulting material reacts under the conditions of being placed in 100~120 DEG C, until low sticky high resiliency colloid of the material in brown, it takes out, with organic solvent washing, shear granulation, drying to get；Wherein: the starch, acrylamide, glycine betaine, initiator and crosslinking agent mass ratio be 1:8~15:2~5:0.15~0.25:0.05~0.1.Oil field sealing agent of the present invention has excellent swelling behavior, the leak stopping especially suitable for high salt concentration water environment.Our experiments show that the water absorbent rate of sealing agent of the present invention is still greater than 30 times in the hypersaline environment that sodium chloride or calcium chloride concentration are 10w/w%.
Description
Technical field
The present invention relates to a kind of oil field sealing agents and preparation method thereof, belong to oilfield chemical technical field.
Background technique
Polyacrylamide and its derivative are widely used in adjusting because yield is big, cheap and thickening effect is obvious
It cuts open, the displacement of reservoir oil, the oil fields such as leak stopping production links.During petroleum drilling and mining, leakage is common down-hole accident, can serious shadow
Ring drilling safety, manufacturing schedule and production cost.Can be had using gel-type polymeric or water swelling quasi polymer sealing agent
Effect prevents leakage.However, the generally existing degradability of conventional sealing agent is poor, problem in high salty formation stability difference, such as " chemistry
Application status of the sealing agent in oil drilling leak-proof leak-stopping " [Ni Yafei, Huang Youliang, Chemical Engineer, 2016,251 (8):
60-62]。
With the progress for improving recovery efficiency technique, the exploitation in high saliferous oil field is inevitable, therefore, develops one kind and is suitable for
The oil field sealing agent of high salt concentration water environment is imperative.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of oil field sealing agents especially suitable for high salt concentration water environment
And preparation method thereof.
Oil field sealing agent of the present invention, shown in structure such as following formula (I):
Wherein, St expression starch, CL expression crosslinking agent, x=0.05~0.08, y=0.65~0.70, z=0.10~
0.20。
The preparation method of above-mentioned oil field sealing agent, it is characterised in that: take starch to be placed in water gelatinization, into gained mixture
Acrylamide and glycine betaine is added, is stirring evenly and then adding into initiator and crosslinking agent, stirs evenly, resulting material is placed in 60~
It is reacted under the conditions of 120 DEG C, until material takes out, with organic solvent washing, shearing is made in the low sticky high resiliency colloid of brown
Grain is dried to get the oil field sealing agent is arrived；Wherein:
The starch, acrylamide, glycine betaine, initiator and crosslinking agent mass ratio be 1:8~15:2~5:0.15~
0.25:0.05~0.1.
In above-mentioned preparation method, the starch is conventional selection in the prior art, is selected from specifically, starch can be
The combination of one or more of potato starch, cereal starch, cornstarch and bean starch etc..Starch is placed in water
The operation of gelatinization is same as the prior art, is usually placed in water starch and is warming up to 80~90 DEG C of 0.5~2h of gelatinization, wherein forming sediment
The mass ratio of powder and water is preferably 1:30~100.
In above-mentioned preparation method, the glycine betaine is the compound with following structures:
In above-mentioned preparation method, the initiator and crosslinking can be conventional selection in the prior art, specifically, drawing
Hair agent can be one in ammonium persulfate, sodium hydrogensulfite, sodium sulfite, potassium peroxydisulfate, ammonium ceric nitrate and ceric sulfate
Kind or two or more combinations, are preferably made of ammonium persulfate, sodium hydrogensulfite and sodium sulfite by the mass ratio of 2:1:0.1
Mixture.The crosslinking agent specifically can be N, N methylene-bisacrylamide, epoxychloropropane or polyethylene glycol acrylic acid
Ester), preferably N, N methylene-bisacrylamide.
In above-mentioned preparation method, material is reacted under the conditions of 60~120 DEG C to logical in the low sticky high resiliency colloid of brown
Often need 10~20min.
In above-mentioned preparation method, the organic solvent specifically can be ethyl alcohol or acetone, can also use ethyl alcohol and acetone
It is sequentially washed in no particular order.
In above-mentioned preparation method, shear granulation carries out usually in pelletizer, and drying is usually dried under the conditions of 50~80 DEG C
It does to moisture content≤1%.
In above-mentioned preparation method, the acrylamide and glycine betaine are preferably added (favorably when system is 85~90 DEG C
In starch gelatinization and reduce the generation of homopolymerization by-product), when the temperature of system is more than above-mentioned temperature, preferably cool to above-mentioned
It is added after temperature range.In order to make acrylamide and glycine betaine spread more evenly across the progress in system in favor of reaction,
Be then added in mixture after preferably dissolving acrylamide and glycine betaine with water, used herein of water dosage be included in front of
In the amount ranges for stating the water of restriction.Mixture is then added to after being dissolved again with water after acrylamide and glycine betaine being mixed
In, it is then added in mixture after acrylamide and glycine betaine can also being dissolved with water respectively.
Compared with prior art, present invention is characterized in that
1, glycine betaine is introduced into molecular resin by the present invention, and gained oil field sealing agent is made to have excellent swelling behavior,
Leak stopping especially suitable for high salt concentration water environment (sodium chloride or calcium chloride concentration reach 10w/w%).The test table of applicant
Bright, in the hypersaline environment that sodium chloride or calcium chloride concentration are 10w/w%, the water absorbent rate of sealing agent of the present invention is still big
In 30 times.On the other hand, the introducing of starch enables gained sealing agent natural degradation.
2, the method for the invention is simple and easy to control, and raw material is easy to get, at low cost, and yield is high.
Detailed description of the invention
Fig. 1 is the infrared spectrum spectrogram of oil field sealing agent made from the embodiment of the present invention 1；
Fig. 2 is the relation curve of oil field sealing agent swelling time and water absorbent rate in salt water of the present invention；
Fig. 3 is that oil field sealing agent of the present invention inhales salt water up to swelling behavior curve when balancing；
Fig. 4 is that oil field sealing agent of the present invention inhales the water retention property curve after salt water.
Specific embodiment
The present invention is described in further detail combined with specific embodiments below, content to better understand the invention, but
The present invention is not limited to following embodiments.
Embodiment 1
250ml three neck round bottom flask is put into oil bath pan, 2g starch (tapioca) and 50g water is added, is warming up to 90
DEG C gelatinization, magnetic agitation, be condensed back 30min after, be cooled to 60 DEG C and keep the temperature；16g acrylamide and 8g glycine betaine is taken to dissolve
In 30g water, acquired solution is added in above-mentioned round-bottomed flask, sequentially adds 0.5g initiator (by persulfuric acid after stirring 10min
The mixture that ammonium, sodium hydrogensulfite and sodium sulfite are formed by the mass ratio of 2:1:0.1) and 0.2g crosslinking agent (N, N di-2-ethylhexylphosphine oxide
Acrylamide), 10min is stirred, system is in slightly viscous pasty state at this time；Resulting material pours into iron pan, is placed in baking oven and is warming up to
Reacted under the conditions of 120 DEG C 10min (at this time material system in brown low sticky high resiliency colloid), take out in time, with largely having
Solvent (ethyl alcohol) washing, be placed in pelletizer and be granulated, white solid granular product is dried to obtain under the conditions of 60 DEG C
26.21g.In the present embodiment, the starch, acrylamide, glycine betaine, initiator, crosslinking agent and water mass ratio be 1:8:4:
0.25:0.1:40；The glycine betaine is the compound with following structures:
The infrared spectroscopy of the present embodiment products therefrom is surveyed using PerkinElmer Frontier FT-IR/FIR spectrometer,
As shown in Figure 1.There is C=C vibration peak (3150cm-1) in the spectrogram, C=O vibration peak (1750cm-1), amide (secondary amine) vibration
Dynamic characteristic peak (1600cm-1), N-H vibration peak (3550cm-1), methyl vibration peak (1400cm-1), methylene vibration peak
(1450cm-1), quaternary ammonium N characteristic peak (1650cm-1), aliphatic amine C-N vibration peak (1100cm-1).Spectrogram demonstrates product
In the presence of.
The degradability that experimental method evaluates the present embodiment products therefrom is buried using soil: product is filled in soil, a timing
Between after take out weighing, calculate weight-loss ratio.Originally 30 days weight-loss ratios for applying a products therefrom are 82.64%.
Embodiment 2
Embodiment 1 is repeated, unlike:
Starch uses cornstarch, and dosage 2g, initiator is ammonium ceric nitrate, and crosslinking agent is epoxychloropropane, You Jirong
Agent is acetone；
Material in iron pan is placed in baking oven the reaction 15min under the conditions of 100 DEG C, and (material system is in the low viscous of brown at this time
Property high resiliency colloid)；
The starch, acrylamide, glycine betaine, initiator, crosslinking agent and water mass ratio be 1:15:2:0.20:0.05:
50。
Finally obtain white solid granular product 26.02g.
Embodiment 3
Embodiment 1 is repeated, unlike:
Starch uses bean starch, and dosage 2g, initiator is ammonium persulfate, and crosslinking agent is polyethylene glycol acrylate；
The acrylamide and glycine betaine do not have to water dissolution and are added directly into round-bottomed flask；
Material in iron pan is placed in baking oven the reaction 20min under the conditions of 110 DEG C, and (material system is in the low viscous of brown at this time
Property high resiliency colloid)；
The starch, acrylamide, glycine betaine, initiator, crosslinking agent and water mass ratio be 1:10:5:0.15:0.08:
30。
Finally obtain white solid granular product 25.95g.
Experimental example 1: sealing agent relationship of swelling time and water absorbent rate in salt water in oil field measures
Under 20 DEG C of environment, respectively in the deionized water of same quality, concentration 10w/w% sodium chloride and concentration 10w/w%
Calcium chloride brine in be added phase homogenous quantities (0.3g) oil field sealing agent of the present invention (press 1 the method system of embodiment
), the water absorbent rate under different soaking times is measured, as a result as shown in Figure 2.
As shown in Figure 2, water absorbent rate tends towards stability after soaking time is more than 5h.In the salt water of 10w/w%, identical leaching
It steeps under time conditions, the water absorbent rate of oil field sealing agent of the present invention is above the numerical value in pure water, therefore, described in invention
Oil field sealing agent have excellent suction salt water effect.
Experimental example 2: oil field sealing agent inhales salt water up to swelling behavior measurement when balancing
Under 20 DEG C of environment, respectively in the calcium chloride salt of the concentration 10w/w% sodium chloride of same quality and concentration 10w/w%
The oil field sealing agent of the present invention (being made by 1 the method for embodiment) of phase homogenous quantities (0.3g) is added in water, impregnates for 24 hours,
Water absorbent rate is measured, as a result as shown in Figure 3.
From the figure 3, it may be seen that oil field sealing agent of the present invention is positively correlated the water absorption and salinity of salt water, to fresh water
Being saturated water absorbent rate is 27.52 times, is 32.19 times to 10w/w% sodium chloride brine, is 31.68 to 10w/w% calcium chloride brine
Times.Illustrate that oil field sealing agent of the present invention has excellent water swelling effect in salt water.
Experimental example 3: oil field sealing agent inhales the water retention property after salt water
It takes by oil field sealing agent made from the embodiment of the present invention 1, is saturated water suction 10w/w% sodium chloride and 10w/w% respectively
It after calcium chloride brine, under 20 DEG C of environment, is respectively placed in loosely capped vial and places certain time, test its water absorbent rate, with saturation
Original state water absorbent rate after absorbing salt water compares, and calculates water retention property, as a result as shown in Figure 4.
As shown in Figure 4, water retention illustrates that oil field of the present invention is stifled 90% or more after after placing in air for 24 hours
Leaking agent has good water retention property.
The above content combination specific embodiment makes further description, but specific implementation of the invention to the present invention
It is not limited to these explanations.For the technical field of the invention, do not depart from present inventive concept under the premise of it is made several
Simple deduction or replace are regarded as belonging to the scope of protection of the present invention.
Claims (10)
1. a kind of oil field sealing agent, shown in structure such as following formula (I):
Wherein, St indicates that starch, CL indicate crosslinking agent, x=0.05~0.08, y=0.65~0.70, z=0.10~0.20.
2. the preparation method of oil field sealing agent described in claim 1, it is characterised in that: take starch to be placed in water gelatinization, to gained
Acrylamide and glycine betaine are added in mixture, is stirring evenly and then adding into initiator and crosslinking agent, stirs evenly, resulting material is set
It is reacted under the conditions of 60~120 DEG C, until material takes out in the low sticky high resiliency colloid of brown, with organic solvent washing, cuts
Granulation is cut, is dried to get the oil field sealing agent is arrived；Wherein:
The starch, acrylamide, glycine betaine, initiator and crosslinking agent mass ratio be 1:8~15:2~5:0.15~0.25:
0.05~0.1.
3. preparation method according to claim 2, it is characterised in that: the starch is to form sediment selected from potato starch, cereal
The combination of one or more of powder, cornstarch and bean starch.
4. preparation method according to claim 2, it is characterised in that: the mass ratio of the starch and water is 1:30~100.
5. preparation method according to claim 2, it is characterised in that: the glycine betaine is the chemical combination with following structures
Object:
6. preparation method according to claim 2, it is characterised in that: the initiator is selected from ammonium persulfate, sulfurous
The combination of one or more of sour hydrogen sodium, sodium sulfite, potassium peroxydisulfate, ammonium ceric nitrate and ceric sulfate.
7. preparation method according to claim 2, it is characterised in that: the initiator is by ammonium persulfate, sulfurous acid
The mixture that hydrogen sodium and sodium sulfite are formed by the mass ratio of 2:1:0.1.
8. preparation method according to claim 2, it is characterised in that: the crosslinking agent is N, N methylene bisacrylamide acyl
Amine, epoxychloropropane or polyethylene glycol acrylate.
9. preparation method according to claim 2, it is characterised in that: the organic solvent is ethyl alcohol and/or acetone.
10. the preparation method according to any one of claim 2-9, it is characterised in that: the acrylamide and beet
Alkali is then added in mixture after being dissolved with water.
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| CN201811197297.XA CN109181661A (en) | 2018-10-15 | 2018-10-15 | A kind of oil field sealing agent and preparation method thereof |
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| CN201811197297.XA CN109181661A (en) | 2018-10-15 | 2018-10-15 | A kind of oil field sealing agent and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102585092A (en) * | 2012-01-16 | 2012-07-18 | 西南石油大学 | Betaine type salt-resistant polymer and preparation method thereof |
| CN104628957A (en) * | 2015-01-23 | 2015-05-20 | 长江大学 | High-strength gel for snubbing operation and preparation method of high-strength gel |
| CN105669499A (en) * | 2016-03-15 | 2016-06-15 | 西南石油大学 | Sulfonate betaine type acrylamide copolymer oil displacement agent and synthesis method thereof |
| CN107814881A (en) * | 2017-11-14 | 2018-03-20 | 西南石油大学 | A kind of quick copolymer gel of temperature sensitive salt and preparation method thereof |
-
2018
- 2018-10-15 CN CN201811197297.XA patent/CN109181661A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102585092A (en) * | 2012-01-16 | 2012-07-18 | 西南石油大学 | Betaine type salt-resistant polymer and preparation method thereof |
| CN104628957A (en) * | 2015-01-23 | 2015-05-20 | 长江大学 | High-strength gel for snubbing operation and preparation method of high-strength gel |
| CN105669499A (en) * | 2016-03-15 | 2016-06-15 | 西南石油大学 | Sulfonate betaine type acrylamide copolymer oil displacement agent and synthesis method thereof |
| CN107814881A (en) * | 2017-11-14 | 2018-03-20 | 西南石油大学 | A kind of quick copolymer gel of temperature sensitive salt and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 王梓民等: "制备接枝共聚羟丙基瓜胶的新工艺 ", 《应用化工》 * |
| 王梓民等: "甜菜碱接枝共聚羟丙基瓜胶的制备 ", 《精细化工》 * |
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